摘要
以叔丁基肼水溶液、糠氯酸为原料,在甲苯做溶剂、冰乙酸做催化剂条件下经成腙、闭环、脱溶,然后在水相结晶制得高含量2-叔丁基-4,5-二氯-3(2H)-哒嗪酮(以下简称哒嗪酮);哒嗪酮再与对叔丁基苄硫醇在甲醇做溶剂的条件下经缩合、脱甲醇、水相结晶制得高含量哒螨灵原药。反应具有操作稳定、收率高的优点,缩合反应在低温下进行,有利于提高产品质量及收率;哒螨灵在一定浓度的稀碱水溶液中结晶,其含量可达到96%以上。该方法具有产品质量高、成本低的优点,适合工业化生产。
With using the tert-butylhydrazine and mucochloric acid as raw materials, the methylbenzene as solvent and the glacial acetic acid as catalyst, the 2-tert-butyl-4,5-dichloro-3 （2H）-pyridazinone （hereinafter referred to as pyridazinone） with high content was got by the processes of hydrazine reaction, ring-closure reaction, desolventizing and crystallization in water. Then the pyridazinone reacted with p-tert-butyl benzyl mercap- tan in methanol solution and the pyridaben active compound with high content was prepared after the processes of condensation reaction, de-methanol reaction and crystallization in water. The reaction was stable with a high yield, the condensation reaction should be carried out at low temperature which would be beneficial to improving the product＇s quality and yield; The content of pyridaben could reach 96% or more after crystallizing in the diluted alkalis solution with a certain concentration. This process was suitable for industrial production which had the advantages of high quality of the product and low cost.
出处
《化学与粘合》
CAS
2014年第6期430-432,437,共4页
Chemistry and Adhesion
关键词
成腙
闭环
哒嗪酮
缩合
高含量
哒螨灵原药
Hydrazine reaction
ring-closure reaction
pyridazinone
condensation reaction
high content
pyridaben active compound
